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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1,2-Dichlorobenzene → 3-(2-chloro-6-fluorophenyl)-5-[3-(3-chloro-5-trifluoromethylpyridine-2-yloxy)-5-methoxyphenyl]-1-methyl-1H-1,2,4-triazole

HRID 52239
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인쇄 미리보기

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HRID 52239 반응식
[CH3:1][N:2](S(C1C=CC(C)=CC=1)(=O)=O)[N:3]=[C:4](Cl)[C:5]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:12].[Cl:24][C:25]1[C:26]([O:35][C:36]2[CH:37]=[C:38]([CH:41]=[C:42]([O:44][CH3:45])[CH:43]=2)[C:39]#[N:40])=[N:27][CH:28]=[C:29]([C:31]([F:34])([F:33])[F:32])[CH:30]=1.ClC1C=CC=CC=1Cl>C(Cl)(Cl)Cl.[Fe](Cl)(Cl)Cl>[Cl:12][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]([F:11])[C:5]=1[C:4]1[N:40]=[C:39]([C:38]2[CH:41]=[C:42]([O:44][CH3:45])[CH:43]=[C:36]([O:35][C:26]3[C:25]([Cl:24])=[CH:30][C:29]([C:31]([F:33])([F:34])[F:32])=[CH:28][N:27]=3)[CH:37]=2)[N:2]([CH3:1])[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 72391,2-DichlorobenzeneHCID 21463661HCID 21463661, 화합물HCID 54347086N-methyl-N-(p-toluenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride

생성물 1

HCID 214635943-(2-chloro-6-fluorophenyl)-5-[3-(3-chloro-5-trifluoromethylpyridine-2-yloxy)-5-methoxyphenyl]-1-methyl-1H-1,2,4-triazole수율 48.7%

시약·촉매·용매 2

HCID 24380
Iron chloride (FeCl3)
촉매
HCID 6212Chloroform용매

반응 조건

온도
140 °C

실험 절차

A mixture of N-methyl-N-(p-toluenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride (0.90 g), 3-(3-chloro-5-trifluoromethylpyridine-2-yloxy)-5-methoxybenzonitrile (0.80 g), anhydrous iron (III) chloride (0.80 g) and o-dichlorobenzene (5 ml) is stirred at an oil bath temperature of 140° C. for 30 minutes. After cooling, it is dissolved in chloroform (100 ml) and washed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline. Then, it is dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography using mixed solvent of hexane-ethyl acetate as eluent to give 0.60 g of desired compound.

후처리

  1. temperatureAfter cooling
  2. washwashed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline
  3. dry with materialThen, it is dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe concentrate is purified by silica gel column chromatography
  6. additionusing mixed solvent of hexane-ethyl acetate as eluent

출처 및 근거

ORD 기록
ord-4003f433d55243c29521e770e2ecc5d0
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05616594

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